Apparatus and method for preparing alcohol from olefin
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Example
Example 1.1
Production of Catalyst Solution
[0082]3.2 kg of triphenyl phosphine (TPP) was completely dissolved in 28.7 kg of normal-butyraldehyde having a purity of 99%. 45.9 g of an acetylacetonatodicarbonyl triphenylphosphine rhodium (ROPAC)) catalyst which had been previously weighted was further added to the solution to prepare 32 kg of a catalyst solution.
Example 1.2
Preparation of Aldehyde and Gas-Liquid Separation
[0083]Referring to FIG. 1, two 30 L loop reactors 100 were produced and a venturi diffusion tube having a nozzle diameter of 5 mm, a diffusion tube inlet diameter of 10 mm, a diffusion tube outlet diameter of 20 mm and a diffusion tube length of 30 mm was mounted on a head of each reactor. In addition, a flat diffusion plate having a diameter of 70 mm was fixed at a position of 200 mm from the lower outlet in the reactor. A circulation pump was mounted in the reactor such that a reaction solution could be recirculated at a flow rate of 20 L / min to a spray nozzle of each...
Example
Example 2
[0096]With reference to FIG. 2, the same process as Example 1 was repeated except that aldehyde suggested in Example 1.2 was gas-liquid separated and was further purified using the same divided wall column (DWC) 700 as in Example 1.4 and separated normal butyraldehyde was fed to the same hydrogenation reactor as in Example 1.3.
[0097]Through startup and stabilization, the separated aldehyde gas-phase substance in Example 1.2 was fed at a flow rate of 6.4 kg / hr to the sixth plate of the pre-column, and the middle-boiling point component was continuously recovered on the twelfth plate from upper and lower parts of the column and the upper part of the main column. A total normal operation time was 86 hours and 1.07 kg of water in total and 20 g or less of iso-butyraldehyde were obtained from the low-boiling point component outlet 710 of the upper part of the column. A three-component mixture containing 47.7 kg of iso-butyraldehyde, 476.6 kg of normal-butyraldehyde and 5 g or le...
Example
Example 3.1
Preparation of Aldehyde Having Increased Number of Carbon Atoms by Aldol Condensation
[0098]With reference to FIG. 3, 20 L of a liquid containing a 2.0% aqueous NaOH solution and normal-butyraldehyde at a ratio of 1:2 was charged in a 30 L vertical continuous stirred tank reactor (CSTR) 500 as an aldol condensation reactor 500 and an inner temperature and pressure of the reactor were maintained at 120° C. and 5 barg, respectively.
[0099]The rate of revolutions was maintained at 300 rpm and the aldehyde mixture prepared in Example 1.3 was subjected to fractional distillation to obtain 240 kg of normal-butyraldehyde having a purity of 99% as a feed for aldol condensation reaction.
[0100]The normal-butyraldehyde thus obtained was continuously fed at a flow rate of 6.3 kg / hr, and a reaction product was recovered using a decanter under normal operation conditions for 32 hours while a liquid level was maintained at 20 liter.
[0101]A weight of the reaction product was 158 kg in tota...
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